CN108732187A - A kind of fast evaluation method of large-area graphene cleanliness factor - Google Patents
A kind of fast evaluation method of large-area graphene cleanliness factor Download PDFInfo
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Abstract
The invention discloses a kind of fast evaluation methods of large-area graphene cleanliness factor.The method of the rapid evaluation large-area graphene cleanliness factor includes the following steps：In such a way that titanium tetrachloride is stifling in graphene sample deposition of titanium oxide nano particle；According to the deposition situation of the titania nanoparticles, that is, realize the assessment to graphene sample cleanliness factor；The stifling condition is as follows：Temperature is 0~30 DEG C；Humidity is 10~70%；Time is 5s~600s；The graphene sample is placed in the top of titanium tetrachloride.Compared with prior art, the beneficial effects of the present invention are：It is of low cost, easy to operate, and can realize and the big face of sample cleanliness factor is quickly characterized.
Description
Technical field
The present invention relates to a kind of fast evaluation methods of large-area graphene cleanliness factor, belong to Material Field.
Background technology
Graphene is a kind of to be arranged the two-dimensional film material formed according to the symmetrical honeycomb structure of six sides by single layer of carbon atom.
Due to the advantageous property that graphene is shown in electricity, optics, calorifics and mechanics etc., just cause since it is found
The extensive concern in each field such as physics, chemistry, biology and material.For example, single-layer graphene has the energy band knot of dirac taper
Structure, at fermi level, energy and the linear dispersion relation of momentum.This unique band structure determines that graphene has pole
High carrier mobility, therefore graphene is increasingly becoming the advantageous replacer of traditional silicon substrate electronic material.Since graphene is
The thin-film material of monoatomic layer, absorptance are only 2.3%, in conjunction with its excellent electric conductivity and flexibility, under graphene becomes
The possibility material of the flexible and transparent conductive material of a generation.
At present chemical vapor deposition method (CVD) be it is quick prepare large area, high-quality graphene thin-film material it is main
Method.However, often there is the pollutant of a large amount of agraphitic carbons, and to stone in graphene surface and unholiness prepared by this method
Excellent light transmittance, electric conductivity and the thermal conductivity of black alkene have adverse effect on.Therefore, it is thin quickly to assess graphene for large area
The cleanliness factor of film becomes particularly important for the application of the optimization of subsequent growth technique and different cleanliness factor graphenes.Mesh
The preceding assessment to the graphene surface cleanliness factor directly grown mostly uses spectrum method and carries out qualitative assessment, such as x-ray photoelectron
Power spectrum, Raman spectrum, infrared spectrum etc., but assessment cycle is long, it is of high cost, and assess limited area.
Invention content
The object of the present invention is to provide a kind of fast evaluation methods of large-area graphene cleanliness factor, and the present invention is based on nanometers
Particle can be with fast transferring in clean graphene surface, and reunion nucleation and growth process is easy at surface contaminant, it is difficult to migration
Principle provides a kind of method of rapid evaluation graphene cleanliness factor.
A kind of method of rapid evaluation large-area graphene cleanliness factor provided by the present invention, includes the following steps：Using
The stifling mode of titanium tetrachloride deposition of titanium oxide nano particle in graphene sample；According to the titania nanoparticles
Deposition situation, that is, realize the assessment to graphene sample cleanliness factor.
In above-mentioned method, the stifling condition is as follows：
Temperature can be 0~30 DEG C, concretely 15~20 DEG C；
Humidity can be 10~70%, concretely 20~40%, 20% or 40%；
Time can be 5s~600s, concretely 10s~60s or 120s.
In above-mentioned method, the graphene sample is placed in the top of titanium tetrachloride, can be surface；
The vapor deposition is carried out in device for fumigation：
The device for fumigation includes beaker and matched Buchner funnel；
The graphene sample is placed in the Buchner funnel；The graphene sample level can be spread in the Bu Shi
The surface of funnel, while it is flat above the steam of the titanium tetrachloride also to control the graphene sample using transmission device
It moves, and then realizes greater area of TiO2The assessment of stifling and cleanliness factor；The graphene sample can also be rolled into multilayer ring-type
It is vertically sprawled along the inner wall of the Buchner funnel or other sprawls mode.
The present invention can realize the adjustment to fumigating area by adjusting the size of the Buchner funnel, such as from 1 × 1cm2It arrives
400cm2Differ.
Can be used visually observe, light microscope (OM), scanning electron microscope (SEM) or transmission electron microscope
(TEM) the graphene sample cleanliness factor is assessed.
Can be by its cleanliness factor of the discoloration qualitative evaluation of the graphene sample, clean graphene is in a certain range
There is no agraphitic carbon adsorbate, therefore there is uniform contrast.
Include bright field image and dark field image to the characterization that titania nanoparticles are distributed using the light microscope, wherein
Especially it is preferred with dark field image.
Under scanning electron microscope or transmission electron microscope observation, according to the uniform realization of contrast to graphene sample
The assessment of cleanliness factor.
The principle of method based on evaluating graphite alkene cleanliness factor of the present invention, the i.e. cleanliness factor of graphene influence nano particle
Distribution, and the distribution density of nano particle and rule have close relationship with its catalytic activity, therefore (utilized through this method
Titania nanoparticles are deposited on graphene by stifling mode) treated, and graphene sample can be used for TiO2Fill-in light
In catalysis.
Compared with prior art, the beneficial effects of the present invention are：It is of low cost, easy to operate, and can realize to sample
The big face of cleanliness factor quickly characterizes.
Description of the drawings
Fig. 1 is the schematic diagram and material object that 1 foam copper of embodiment of the present invention auxiliary realizes prepared by the magnanimity of ultra-clean graphene
Figure.
Fig. 2 is the typical TEM characterization results of ultra-clean graphene prepared by 1 foam copper of embodiment of the present invention auxiliary.
Fig. 3 is that 1 titanium tetrachloride of the embodiment of the present invention fumigates selective deposition titanium dioxide granule realization graphene cleanliness factor
The exemplary device of assessment.
Fig. 4 is the allusion quotation of 1 titanium dioxide fumigating system large area rapid evaluation ultra-clean graphene cleanliness factor of the embodiment of the present invention
Type experimental result.
Fig. 5 is that the TEM that the graphene that in the embodiment of the present invention 2 prepared by common process obtains after clean shift characterizes knot
Fruit, growth temperature from left to right are followed successively by 900 DEG C, 950 DEG C and 1040 DEG C.
Fig. 6 is the selectivity of hanging graphene its surface titanium dioxide after titanium tetrachloride is stifling in the embodiment of the present invention 2
Deposition and the regularity of distribution, wherein left figure are that the typical high power transmitted electron of carbon dioxide nano particle distribution on hanging graphene is aobvious
Micro mirror picture, right figure are the corresponding energy spectrum analysis in the region.
Fig. 7 is the cleanliness factor assessment that 2 titanium dioxide fumigating system of embodiment of the present invention auxiliary realizes common graphite alkene sample.
Specific implementation mode
Experimental method used in following embodiments is conventional method unless otherwise specified.
The materials, reagents and the like used in the following examples is commercially available unless otherwise specified.
The cleanliness factor of embodiment 1, the ultra-clean graphene using the method that titanium tetrachloride is fumigated prepared by foam copper auxiliary
It is assessed
(1) dilute hydrochloric acid and deionized water that use quality score is 5% clean copper foil successively, and (Alfa Aesar companies give birth to
Production, purity 99.8%, 25 μm of thickness), copper foil and foam copper are in close contact (it is specifically the top that foam copper is placed in copper foil, it
Between spacing be 0.01~1mm, as shown in Figure 1) be placed in the casing with magnetic force control device, then casing is placed in tube furnace
In, in the case where flow is the hydrogen atmosphere of 100sccm, system pressure is 100Pa, and furnace body temperature is risen to 1020 DEG C, is kept
30min；
(2) furnace body temperature is maintained at 1020 DEG C, changes hydrogen and be passed through the hydrogen gas that flow is 11sccm, is passed through flow
For the methane gas of 7sccm, system pressure is 50Pa, keeps 30s；
(3) it uses magnet to haul out the casing for loading copper foil from high-temperature region, sample temperature is rapidly decreased to room temperature, cooling speed
Rate is 90 DEG C/min, terminates sample grown；
(4) copper foil sample that growth finishes is taken out, be cut into suitably sized or is sampled according to equidistantly multiple, by graphite
Alkene sample is placed on right over titanium tetrachloride vapors (being carried out in device as shown in Figure 3), and controlling reaction temperature is 15 DEG C, air
Humidity is 40%, after fumigating 10~60s, observes the discoloration of copper foil surface and counts the distribution density of titanium dioxide.Simultaneously
Sample cleaning is transferred in transmission contained network to facilitate its cleanliness factor of quantitative assessment.
Fig. 1 is the schematic diagram and pictorial diagram that foam copper auxiliary realizes prepared by the magnanimity of ultra-clean graphene.Wherein, foam copper
Spacing control between copper foil influences the graphene cleanliness factor of preparation very big.Using this method, continuous surface can be once prepared
Product is more than 10 × 100cm2Ultra-clean graphene sample.
Fig. 2 is the allusion quotation that ultra-clean graphene prepared by the present embodiment foam copper auxiliary carries out TEM characterizations after no glue shifts
Type result.Color is deeper agraphitic carbon adsorbate caused by growth under transmission electron microscope, and ultra-clean manufactured in the present embodiment
Graphene film does not have the distribution of such adsorbate, clean graphene to show uniform contrast in the range of continuous 1 micron,
Illustrate that contamination-free adsorbs, it was demonstrated that the continuous cleaning area of graphene manufactured in the present embodiment reaches micro-meter scale.And unskilled labor
Graphene sample prepared by skill, continuous cleaning area is only several nanometers to several tens of nanometers.
Fig. 3 is the reality for carrying out the stifling selective deposition for realizing titania nanoparticles on the surface of graphene of titanium tetrachloride
Experiment device.In specific experiment, Hygrothermograph provides experiment condition and assists the fumigation time of adjustment titanium tetrachloride vapors；Copper foil ruler
Very little size can be come matching by adjusting the size of beaker and Buchner funnel.The placement of copper foil can be as shown in Figure 3, is rolled into
Ring-type along inner wall of hopper place, can also be rolled into it is polycyclic be placed in funnel, can also remove funnel directly right over it fumigate.
Fig. 4 is the large area that the ultra-clean graphene that the embodiment of the present invention is prepared utilizes titanium dioxide fumigating system to realize
The model experiment of rapid evaluation graphene cleanliness factor it can be seen from left figure as a result, once assess area up to 20 × 20cm2With
On.Due to graphene surface cleaning, the substantially not no selective deposition of titanium dioxide granule, therefore copper foil surface is smooth, color and luster
It does not change.Similarly, as shown on the right, the ultra-clean graphene prepared to batch, samples every 10cm and fumigates four chlorinations
Titanium steam has counted the number of titanium dioxide granule in unit area, finds numerical value perseverance less than 20, and the graphite of common cleanliness factor
Alkene sample, the number of nano particle is up to more or less a hundred in equal area.
Embodiment 2, the graphene using the method that titanium tetrachloride is fumigated prepared by common CVD techniques cleanliness factor comment
Estimate
(1) it is 3 to use volume ratio：1 phosphoric acid and ethylene glycol solution is as electrolyte, by copper foil (Alfa Aesar companies
Production, purity 99.8%, 25 μm of thickness) connect positive, polishing treatment 30min under DC current 0.5A.Copper foil is placed in and is carried
In the casing of magnetic force control device, then casing is placed in tube furnace, in the case where flow is the hydrogen atmosphere of 300sccm, by furnace body
Temperature rises to 1000 DEG C, and system pressure is 300Pa, keeps 50min.
(2) furnace body temperature is maintained at 900 DEG C, 950 DEG C or 1040 DEG C, changes hydrogen and is passed through the hydrogen that flow is 500sccm
Gas gas is passed through the methane gas that flow is 1sccm, and system pressure is about 500Pa, keeps 8h.
(3) it uses magnet to haul out the casing for loading copper foil from high-temperature region, sample temperature is rapidly decreased to room temperature, terminates sample
Product are grown.
(4) copper foil sample that growth finishes is taken out, be cut into suitably sized or is sampled according to equidistantly multiple, by graphite
Alkene sample is placed on right over carbon tetrachloride steam, and controlling reaction temperature is 15 DEG C, air humidity 40%, after fumigating 10~60s,
It observes the discoloration of copper foil surface and counts the distribution density of titanium dioxide.Sample cleaning is transferred in transmission contained network simultaneously
To facilitate by its cleanliness factor of assessment more quantitative TEM.Hanging graphene sample equally sees its distribution with titanium tetrachloride is stifling.
Fig. 5 is typical TEM characterization result of the graphene sample of common CVD techniques preparation after no glue cleaning transfer, from
Left-to-right growth temperature is followed successively by 900 DEG C, 950 DEG C and 1040 DEG C, and the wherein deeper region of contrast has a large amount of amorphous carbon miscellaneous
The enrichment of matter, corresponding continuous cleaning area is respectively 0~5nm, 10~30nm and 50~100nm from left to right；It is corresponding clean
Net area proportion is respectively<30%, 30~50% and>40~60%, it is seen then that can be by adjusting carbon source kind, growth temperature
Degree and copper foil modes of emplacement etc. realize that the preparation of different cleanliness factor graphenes, the present embodiment use the side for adjusting growth temperature
Formula.
Fig. 6 is the distribution of common graphite alkene titania nanoparticles after titanium tetrachloride is stifling, it is found that nanometer
Grain is prevalent in amorphous carbon distributed areas, and the distribution of distribution profile and amorphous carbon essentially coincides.Due to Ti atom matter
Amount is big, shows as deeper contrast under the tem.Nano particle crystallinity is poor, mostly amorphous substance.Meanwhile in conjunction with element
It analyzes (right figure), it is thus identified that the selective distribution (being the dense distribution of titanium dioxide at black particle) of titanium dioxide granule.Card
The stifling reliability for realizing graphene cleanliness factor rapid evaluation of titanium tetrachloride is illustrated.
Fig. 7 is the model experiment knot after graphene sample rapid large-area development prepared by the common CVD techniques of the present embodiment
Fruit.Since the selective deposition of titania nanoparticles is more, there is apparent discoloration, and color and unevenness in copper foil surface
One.To such sample by dark field optical microscope characterization it can be found that the dense distribution of titanium dioxide granule, distribution density
Corresponding to the green point in Fig. 4, hence it is evident that be more than the distribution density of ultra-clean sample surfaces titanium dioxide.Further demonstrate four chlorinations
The stifling reliability for realizing graphene cleanliness factor rapid evaluation of titanium.
The stifling method of carbon tetrachloride of the present invention can qualitative more different cleanliness factor samples when large area assesses cleanliness factor
The otherness of product.
Embodiment 3, the graphene using the method that titanium tetrachloride is fumigated prepared by common CVD techniques cleanliness factor comment
Estimate
(1) it is 3 to use volume ratio：1 phosphoric acid and ethylene glycol solution is as electrolyte, by copper foil (Alfa Aesar companies
Production, purity 99.8%, 25 μm of thickness) connect positive, polishing treatment 30min under DC current 0.5A.Copper foil is placed in and is carried
In the casing of magnetic force control device, then casing is placed in tube furnace, in the case where flow is the hydrogen atmosphere of 300sccm, by furnace body
Temperature rises to 1000 DEG C, and system pressure is 300Pa, keeps 50min.
(2) furnace body temperature is maintained at 1000 DEG C, changes hydrogen and be passed through the hydrogen gas that flow is 500sccm, is passed through stream
Amount is the methane gas of 1sccm, and system pressure is about 500Pa, keeps 8h.
(3) it uses magnet to haul out the casing for loading copper foil from high-temperature region, sample temperature is rapidly decreased to room temperature, terminates sample
Product are grown.
(4) copper foil sample that growth finishes is taken out, be cut into suitably sized or is sampled according to equidistantly multiple, by graphite
Alkene sample is placed on right over carbon tetrachloride steam, and controlling reaction temperature is 20 DEG C, air humidity 20%, after fumigating 120s, is seen
It examines the discoloration of copper foil surface and counts the distribution density of titanium dioxide.Simultaneously by sample cleaning be transferred to transmission contained network on
Conveniently by its cleanliness factor of assessment more quantitative TEM.Hanging graphene sample equally sees its distribution with titanium tetrachloride is stifling.
The typical TEM characterization results of graphene sample prepared by the common CVD techniques of the present embodiment after no glue cleaning transfer
With Fig. 5 without substantial differences, it can be seen that graphene continuous cleaning area very little, clean area occupied area ratio are generally small
In 50%.
Point of the graphene that the present embodiment is prepared through common CVD techniques titania nanoparticles after titanium tetrachloride is stifling
Cloth and Fig. 6 are without substantial differences, it is found that nano particle is prevalent in amorphous carbon distributed areas, distribution profile with
The distribution of amorphous carbon essentially coincides.Since Ti atomic masses are big, deeper contrast is shown as under the tem.Nano particle crystallizes
Property is poor, mostly amorphous substance.Meanwhile in conjunction with elemental analysis, it is thus identified that the selective distribution of titanium dioxide granule.It demonstrates
The stifling reliability for realizing graphene cleanliness factor rapid evaluation of titanium tetrachloride.Graphene prepared by the common CVD techniques of the present embodiment
Model experiment result after the development of sample rapid large-area, without substantial differences, it is stifling to further demonstrate titanium tetrachloride with Fig. 7
Realize the reliability of graphene cleanliness factor rapid evaluation.
Comparative example 1, the graphene using the method that titanium tetrachloride is fumigated prepared by common CVD techniques cleanliness factor comment
Estimate
(1)-(3) the CVD preparation processes of graphene are the same as embodiment 2.
(4) copper foil sample that growth finishes is taken out, be cut into suitably sized or is sampled according to equidistantly multiple, by graphite
Alkene sample is placed on right over carbon tetrachloride steam, and controlling reaction temperature is 60 DEG C, air humidity 100%, after fumigating 60s, is seen
It examines the discoloration of copper foil surface and counts the distribution density of titanium dioxide.
In above-mentioned experiment, too acutely (temperature is too high, and humidity is too big) due to reaction condition, cause titanium tetrachloride rapidly and water
Vigorous reaction, generates prodigious particulate matter, and the regularity of distribution and density can not effectively reflect graphene cleanliness factor.This comparative example
Further illustrate the importance and necessity of reaction condition control.
The stifling method of carbon tetrachloride of the present invention can qualitative more different cleanliness factor samples when large area assesses cleanliness factor
The otherness of product.
Claims (9)
1. a kind of method of rapid evaluation large-area graphene cleanliness factor, includes the following steps：The side fumigated using titanium tetrachloride
Formula deposition of titanium oxide nano particle in graphene sample；According to the deposition situation of the titania nanoparticles, i.e., in fact
Now to the assessment of graphene sample cleanliness factor.
2. according to the method described in claim 1, it is characterized in that：The stifling condition is as follows：
Temperature is 0~30 DEG C；
Humidity is 10~70%；
Time is 5s~600s.
3. method according to claim 1 or 2, it is characterised in that：The graphene sample is placed in the upper of titanium tetrachloride
Side.
4. method according to any one of claim 1-3, it is characterised in that：The vapor deposition is carried out in device for fumigation：
The device for fumigation includes beaker and matched Buchner funnel；
The graphene sample is placed in the Buchner funnel.
5. according to the method described in claim 4, it is characterized in that：The graphene sample is spread in into the Buchner funnel
On inner wall.
6. according to the method described in claim 5, it is characterized in that：The graphene sample is rolled into multilayer ring-type along the cloth
The inner wall of family name's funnel is vertically sprawled.
7. according to the method described in claim 4, it is characterized in that：The graphene sample level is spread in into the Bu Shi leakages
The surface of bucket.
8. according to the method described in claim 7, it is characterized in that：The graphene sample is controlled described using transmission device
Translation above the steam of titanium tetrachloride.
9. according to the method described in any one of claim 1-8, it is characterised in that：Using visually observe, light microscope or
Scanning electron microscope assesses the graphene sample cleanliness factor.
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